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The PL spectra of solid solutions in the PbF2-EuF3 system were studied. Samples were obtained by coprecipitation from aqueous solutions and sintering in a solid state. The study of photoluminescence spectra of single-phase samples showed a more crystalline and more symmetrical structure for samples obtained by coprecipitation with additional heat treatment. Samples obtained by solid-phase synthesis are more centrosymmetric than those obtained by coprecipitation. In general, solid solutions of fluorite type Pb1-xEuxF2+x are characterized by a high degree of symmetry.